CN112033927B - Detection method for ion conductivity of solid electrolyte - Google Patents
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- 239000007784 solid electrolyte Substances 0.000 title claims abstract description 102
- 238000001514 detection method Methods 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 26
- 238000001328 terahertz time-domain spectroscopy Methods 0.000 claims abstract description 19
- 238000012360 testing method Methods 0.000 claims abstract description 13
- 150000002500 ions Chemical class 0.000 claims description 23
- 238000006073 displacement reaction Methods 0.000 claims description 20
- 238000001228 spectrum Methods 0.000 claims description 15
- 230000003287 optical effect Effects 0.000 claims description 11
- 230000005540 biological transmission Effects 0.000 claims description 6
- 230000031700 light absorption Effects 0.000 claims description 5
- 239000010409 thin film Substances 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 2
- 239000004065 semiconductor Substances 0.000 claims description 2
- 239000002203 sulfidic glass Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 7
- 238000005259 measurement Methods 0.000 abstract description 7
- 238000011161 development Methods 0.000 abstract description 4
- 238000003466 welding Methods 0.000 abstract description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 6
- 229910052744 lithium Inorganic materials 0.000 description 6
- SKJCKYVIQGBWTN-UHFFFAOYSA-N (4-hydroxyphenyl) methanesulfonate Chemical compound CS(=O)(=O)OC1=CC=C(O)C=C1 SKJCKYVIQGBWTN-UHFFFAOYSA-N 0.000 description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011244 liquid electrolyte Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3581—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using far infrared light; using Terahertz radiation
- G01N21/3586—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using far infrared light; using Terahertz radiation by Terahertz time domain spectroscopy [THz-TDS]
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/41—Refractivity; Phase-affecting properties, e.g. optical path length
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Abstract
The invention discloses a detection method of ion conductivity of a solid electrolyte, which comprises the steps of preparing a solid electrolyte sheet, testing the solid electrolyte sheet by using a terahertz time-domain spectroscopy system, and calculating to obtain the ion conductivity of the solid electrolyte; the method further comprises the steps of carrying out two-dimensional scanning on the solid electrolyte thin sheet by using a terahertz time-domain spectroscopy system to obtain an ion conductivity two-dimensional image of the solid electrolyte, and evaluating the ion conductivity of the solid electrolyte by analyzing the ion conductivity and the ion conductivity two-dimensional image of the solid electrolyte. The invention is used as a non-contact measurement mode, avoids various problems caused by poor welding in electrical measurement, and can more accurately and more efficiently obtain the ionic conductivity of the solid electrolyte; the invention also obtains a two-dimensional image of the conductivity of the material by adopting a two-dimensional scanning mode, thereby being capable of checking the consistency of the material and helping to analyze the performance of the material. The measuring method can efficiently and accurately compare and analyze the ion conductivity of the solid electrolyte, and provides reliable reference data for the development of the solid electrolyte.
Description
Technical Field
The invention relates to the technical field of lithium batteries, in particular to a detection method for ionic conductivity of a solid electrolyte.
Background
Compared with the traditional liquid electrolyte lithium ion battery, the all-solid-state lithium ion battery has the following advantages: the battery pack has high safety/thermal stability, an electrochemical window of more than 5V, can be matched with a high-voltage material, only conducts lithium ions and does not conduct electrons, and can be connected in series to form a high-voltage single battery, but the battery pack also has the problems to be solved: the interface impedance between the electrode and the electrolyte is large, and the multiplying power performance is poor; the ionic conductivity of unit area is low, and the specific power is poor at normal temperature; high cost and great difficulty in industrialized production of large-capacity batteries.
With the development and popularization of the industry, people further improve the requirements of lithium battery performances, such as high energy density, safety performance, service life and the like. From the viewpoint of safety and high energy density, the all-solid-state lithium battery will have a huge market in the future in the fields of portable electronic devices, medical devices, toys, electric vehicles, and the like.
For all-solid-state lithium batteries, the solid electrolyte is a key, and needs to meet the requirements of high ionic conductivity, good mechanical properties, chemical compatibility and the like. A major focus of future research into all solid-state lithium batteries is to further increase the ionic conductivity of the solid-state electrolyte. Therefore, it is important to develop a fast and efficient method for measuring, comparing and analyzing the ionic conductivity of solid electrolytes.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a method for detecting the ionic conductivity of a solid electrolyte, which is used for quickly and effectively measuring, comparing and analyzing the ionic conductivity of the solid electrolyte.
The invention provides a method for detecting ion conductivity of a solid electrolyte, which comprises the following steps: preparing a solid electrolyte thin film, testing the solid electrolyte thin film by using a terahertz time-domain spectroscopy system to obtain a terahertz time-domain spectrum of terahertz transmission intensity-time, performing Fourier transform on the terahertz time-domain spectrum to obtain a terahertz frequency-domain spectrum of terahertz transmission intensity-frequency, extracting the refractive index and the light absorption coefficient of the solid electrolyte according to the terahertz frequency-domain spectrum, calculating to obtain complex conductivity, and fitting the complex conductivity by using a Drude model to obtain the ionic conductivity of the solid electrolyte.
Preferably, the method for detecting the ion conductivity of the solid electrolyte further comprises the steps of performing two-dimensional scanning on the solid electrolyte sheet by using a terahertz time-domain spectroscopy system to obtain a two-dimensional image of the ion conductivity of the solid electrolyte, and evaluating the consistency of detection of the ion conductivity; if the two-dimensional image is high in uniformity, the detection consistency is good; otherwise, the detection consistency is poor.
Preferably, formulas for extracting the refractive index and the light absorption coefficient of the solid electrolyte according to the terahertz frequency domain spectrum are respectively shown as formula (1) and formula (2):
wherein n is the refractive index, k is the absorption coefficient, A is the intensity,
is the phase, w is the frequency, d is the solid electrolyte sheet thickness, c is the speed of light; the formula (1) and the formula (2) are obtained through a Fresnel equation and a boundary condition;
the complex conductivity is calculated as shown in formula (3):
wherein epsilon 0 Is the absolute dielectric constant, i is the imaginary unit, σ is the complex conductivity, n is the index of refraction, k is the absorptivity, w is the frequency;
the Drude model formula adopted for fitting the complex conductivity is shown as the formula (4):
wherein sigma 0 For ionic conductivity and gamma for transport scatteringThe ratio, i is an imaginary unit, and w is the frequency.
Preferably, the method for detecting the ion conductivity of the solid electrolyte comprises the following steps:
s1, preparing the solid electrolyte into a solid electrolyte sheet;
s2, building a test light path of the terahertz time-domain spectroscopy system, generating terahertz light spots, and focusing and positioning the terahertz light spots;
s3, fixing the solid electrolyte sheet on a multi-dimensional displacement system through a clamp;
s4, adjusting the position of the solid electrolyte sheet through a multidimensional displacement system to enable the solid electrolyte sheet to be located at the focus of the terahertz light spot, and enabling the surface of the solid electrolyte sheet to be perpendicular to the terahertz light spot;
s5, testing the solid electrolyte thin film by using a terahertz time-domain spectroscopy system to obtain a terahertz time-domain spectrum of terahertz transmission intensity-time, performing Fourier transform on the terahertz time-domain spectrum to obtain a terahertz frequency-domain spectrum of terahertz transmission intensity-frequency, extracting the refractive index and the light absorption coefficient of the solid electrolyte according to the terahertz frequency-domain spectrum, calculating to obtain complex conductivity, and fitting the complex conductivity by using a Drude model to obtain the ionic conductivity of the solid electrolyte;
and S6, performing two-dimensional scanning on the solid electrolyte sheet by using a terahertz time-domain spectroscopy system to obtain an ion conductivity two-dimensional image of the solid electrolyte.
Preferably, the diameter of the focused terahertz light spot is 30-500 mu m, and the ion conductivity two-dimensional image resolution of the solid electrolyte is 300-500 mu m.
Preferably, the solid electrolyte thin sheet is fixed on a two-dimensional displacement platform of the multi-dimensional displacement system through a clamp, and the precision of the two-dimensional displacement platform is 1-10 μm.
Preferably, the generation method of the terahertz light spot is an optical rectification method, a semiconductor instant current generation method or an accelerated electron generation method.
Preferably, in step S6, when the terahertz time-domain spectroscopy system performs two-dimensional scanning, a horizontal optical path or a vertical optical path is adopted.
Preferably, the solid electrolyte is a sulfide solid electrolyte, an oxide solid electrolyte or a polymer solid electrolyte.
Preferably, the ion conductivity of the solid electrolyte is evaluated by analyzing its ion conductivity and ion conductivity two-dimensional images.
Preferably, the solid electrolyte is Li 10 GeP 2 S 12 、Li 7 La 3 Zr 2 O 12 Or a polyethylene oxide (PEO) based solid electrolyte.
Preferably, the thickness of the solid electrolyte thin sheet is 0.5 to 1 mm.
The invention has the following beneficial effects:
(1) according to the testing method, a non-contact terahertz time-domain spectroscopy optical measuring means is adopted, so that the measuring problems caused by the welding problems of insufficient welding, poor welding spots and the like in the traditional electrical measuring means are avoided, the conductivity information of different solid electrolytes is effectively obtained, and the data obtained through comparison and analysis provides a high-efficiency measuring and developing auxiliary means for optimizing and developing the all-solid-state lithium battery;
(2) the test method of the invention provides a two-dimensional scanning measurement mode, avoids measurement errors possibly caused by non-uniform materials, and can obtain accurate material conductivity information; meanwhile, the relation between the material structure and the conductivity can be obtained according to the result of the two-dimensional scanning, and reliable reference data is provided for the development of the solid electrolyte; the measuring mode also has the advantage of wide application range, and the measurement can be carried out only by making the solid electrolyte into a thin sheet.
Drawings
Fig. 1 is a schematic diagram of a test optical path of a terahertz time-domain spectroscopy system.
FIG. 2 is a schematic diagram of a multi-dimensional displacement system.
FIG. 3 shows the measured ionic conductivities of various solid electrolytes in example 1 of the present invention.
Detailed Description
As shown in fig. 1, fig. 1 is a schematic diagram of a test optical path of a terahertz time-domain spectroscopy system.
Referring to fig. 1, terahertz light is generated by adopting an optical rectification effect of ultrafast laser, and is detected by combining an electro-optical sampling method. Ultra-short pulse laser with the pulse width of 100 femtoseconds is adopted as a light source, and is split by a beam splitting plate, and one beam of light is converged as a pumping source and is irradiated to zinc telluride (ZnTe) 2 ) Terahertz light is generated on the crystal, and then is focused to a sample position through the metal parabolic mirror for measurement; the other beam of light is used as detection light, and the optical delay between the other beam of light and the pump light is adjusted through an optical delay line; finally, the terahertz light and the detection light are converged and hit another ZnTe 2 On the crystal, detection light passes through a Wrenst prism to obtain horizontal and vertical polarized light, and the horizontal and vertical polarized light enters a detector. Before measurement, the reading of the detector is adjusted to be zero, and when terahertz light is emitted to ZnTe for detection 2 On the crystal, the polarization property of the crystal is changed, so that the polarization property of the detection light is changed, and the detection of the terahertz light by an electro-optical sampling method is realized.
Referring to fig. 2, fig. 2 is a schematic diagram of a multidimensional displacement system. The bottom of the multidimensional displacement system is provided with a manual two-dimensional adjusting device to realize the adjustment of the horizontal position; a lifting platform is fixed above the manual two-dimensional adjusting device and used for adjusting the height; a vertical framework similar to a mirror frame is arranged above the lifting platform, the two-dimensional displacement platform fixed with the sample is arranged on the vertical framework, and pitching and tilting adjustment of the two-dimensional displacement platform can be realized through the vertical framework so as to ensure that the incident terahertz light spot is vertical to the sample surface; the sample is fixed on the two-dimensional displacement platform through the clamp, so that the multidimensional fine adjustment of the position of the sample is realized.
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
For solid electrolyte Li respectively 10 GeP 2 S 12 Solid electrolyte Li 7 La 3 Zr 2 O 12 PEO-based solid electrolyte was subjected to an ionic conductivity test, the procedure was as follows:
s1, preparing the solid electrolyte into a sheet with the thickness of 1 mm;
s2, building a test light path of the terahertz time-domain spectroscopy system, generating terahertz light spots, and focusing and positioning the terahertz light spots;
s3, fixing the solid electrolyte thin sheet on a two-dimensional displacement platform of the multi-dimensional displacement system through a clamp;
s4, adjusting the position of the solid electrolyte sheet through a multidimensional displacement system to enable the solid electrolyte sheet to be located at the focus of the terahertz light spot, and enabling the surface of the solid electrolyte sheet to be perpendicular to the terahertz light spot;
s5, testing the solid electrolyte thin film by using a terahertz time-domain spectroscopy system to obtain a terahertz time-domain spectrum, obtaining a terahertz frequency-domain absorption spectrum by adopting fast Fourier transform, extracting according to formulas (1) and (2) respectively according to the terahertz frequency-domain absorption spectrum to obtain the refractive index and the absorption coefficient of the solid electrolyte, calculating according to a formula (3) to obtain the complex conductivity of the solid electrolyte, and fitting the obtained complex conductivity by adopting a Drude model formula shown in a formula (4) to obtain the ionic conductivity of the solid electrolyte:
wherein n is the refractive index, k is the absorption coefficient, A is the intensity,
is the phase, w is the frequency, d is the thickness of the sheet, c is the speed of light, ε 0 Is the absolute dielectric constant, i is the imaginary unit, σ is the complex conductivity, σ 0 Is the ionic conductivity, and gamma is the transport scattering rate;
and S6, performing two-dimensional scanning on the solid electrolyte sheet by using a terahertz time-domain spectroscopy system to obtain an ion conductivity two-dimensional image of the solid electrolyte.
The diameter of the focused terahertz light spot is 50 micrometers, the precision of the two-dimensional displacement platform is 1 micrometer, and the ion conductivity two-dimensional image resolution of the solid electrolyte is 300 micrometers.
Testing of solid electrolyte Li Using the method described above 10 GeP 2 S 12 Solid electrolyte Li 7 La 3 Zr 2 O 12 The ionic conductivity results of the PEO-based solid electrolyte are shown in fig. 3. As can be seen from FIG. 3, the test method can well reflect the difference of ion conductivity of different solid electrolytes, and provides important reference data for further development and optimization of the solid electrolytes.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (8)
1. A method for detecting ion conductivity of a solid electrolyte is characterized by comprising the following steps:
s1, preparing the solid electrolyte into a solid electrolyte sheet;
s2, building a test light path of the terahertz time-domain spectroscopy system, generating terahertz light spots, and focusing and positioning the terahertz light spots;
s3, fixing the solid electrolyte sheet on a multi-dimensional displacement system through a clamp;
s4, adjusting the position of the solid electrolyte sheet through a multidimensional displacement system to enable the solid electrolyte sheet to be located at the focus of the terahertz light spot, and enabling the surface of the solid electrolyte sheet to be perpendicular to the terahertz light spot;
s5, testing the solid electrolyte thin film by using a terahertz time-domain spectroscopy system to obtain a terahertz time-domain spectrum of terahertz transmission intensity-time, performing Fourier transform on the terahertz time-domain spectrum to obtain a terahertz frequency-domain spectrum of terahertz transmission intensity-frequency, extracting the refractive index and the light absorption coefficient of the solid electrolyte according to the terahertz frequency-domain spectrum, calculating to obtain complex conductivity, and fitting the complex conductivity by using a Drude model to obtain the ionic conductivity of the solid electrolyte;
s6, performing two-dimensional scanning on the solid electrolyte sheet by using a terahertz time-domain spectroscopy system to obtain an ion conductivity two-dimensional image of the solid electrolyte;
formulas for extracting the refractive index and the light absorption coefficient of the solid electrolyte according to the terahertz frequency domain spectrum are respectively shown as formula (1) and formula (2):
wherein n is the refractive index, k is the absorption coefficient, A is the intensity,
is the phase, w is the frequency, d is the sheet thickness, c is the speed of light;
the complex conductivity is calculated as shown in formula (3):
wherein epsilon 0 Is the absolute dielectric constant, i is the imaginary unit, σ is the complex conductivity, n is the index of refraction, k is the absorptivity, w is the frequency;
the Drude model formula adopted for fitting the complex conductivity is shown as the formula (4):
wherein sigma 0 Is the ionic conductivity, gamma is the transport scattering power, i is the imaginary unit, and w is the frequency.
2. The method for detecting ionic conductivity of a solid electrolyte according to claim 1, further comprising: performing two-dimensional scanning on the solid electrolyte sheet by using a terahertz time-domain spectroscopy system to obtain an ion conductivity two-dimensional image of the solid electrolyte, and evaluating the consistency of ion conductivity detection; if the two-dimensional image has high uniformity, the detection consistency is good; otherwise, the detection consistency is poor.
3. The method for detecting the ion conductivity of the solid electrolyte according to claim 1, wherein the diameter of the focused terahertz light spot is 30-500 μm, and the ion conductivity two-dimensional image resolution of the solid electrolyte is 300-500 μm.
4. The method for detecting ionic conductivity of a solid electrolyte according to any one of claims 1 to 3, wherein the solid electrolyte sheet is fixed on a two-dimensional displacement platform of a multidimensional displacement system by a clamp, and the precision of the two-dimensional displacement platform is 1 to 10 μm.
5. The method for detecting the ionic conductivity of the solid electrolyte according to any one of claims 1 to 4, wherein the terahertz light spot is generated by a light rectification method, a semiconductor instant current generation method or an accelerated electron generation method.
6. The method for detecting the ionic conductivity of the solid electrolyte according to any one of claims 1 to 5, wherein in the step S6, when the terahertz time-domain spectroscopy system is used for two-dimensional scanning, a horizontal optical path or a vertical optical path is adopted.
7. The method for detecting ionic conductivity of a solid electrolyte according to any one of claims 1 to 6, further comprising: the ion conductivity of the solid electrolyte was evaluated by analyzing its ion conductivity and ion conductivity two-dimensional images.
8. The method for detecting the ionic conductivity of the solid electrolyte according to any one of claims 1 to 7, wherein the solid electrolyte is a sulfide solid electrolyte, an oxide solid electrolyte or a polymer solid electrolyte; the thickness of the solid electrolyte sheet is 0.5-1 mm.
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